Systems and methods for making ceramic powders

ABSTRACT

Systems and methods for making ceramic powders configured with consistent, tailored characteristics and/or properties are provided herein. In some embodiments a system for making ceramic powders, includes: a reactor body having a reaction chamber and configured with a heat source to provide a hot zone along the reaction chamber; a sweep gas inlet configured to direct a sweep gas into the reaction chamber and a sweep gas outlet configured to direct an exhaust gas from the reaction chamber; a plurality of containers, within the reactor body, configured to retain at least one preform, wherein each container is configured to permit the sweep gas to flow therethrough, wherein the preform is configured to permit the sweep gas to flow there through, such that the precursor mixture is reacted in the hot zone to form a ceramic powder product having uniform properties.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of International Patent ApplicationNo. PCT/US2017/041057, filed Jul. 7, 2017, which claims benefit of U.S.provisional application No. 62/360,079, filed Jul. 8, 2016, each ofwhich is herein incorporated by reference in its entirety.

FIELD OF THE INVENTION

Broadly, the invention relates to systems and methods of making ceramicpowders. More specifically, the present disclosure relates tocarbothermically synthesizing various ceramic powders in a continuousreactor such that the resulting ceramic powder product is configuredwith consistent, tailored characteristics and/or properties.

BACKGROUND

Through carbothermic synthesis, it is possible to make various boride,nitride, and/or carbide ceramic powders. The ceramic powders can then beprocessed into final ceramic products for a wide variety ofapplications.

SUMMARY OF THE INVENTION

In one aspect of the instant disclosure, a system comprises: a reactorbody having a first end and a second end, wherein the reactor body isconfigured with an inner sidewall extending from the first end to thesecond end to define a reaction chamber; wherein the reactor body isconfigured with a heat source to provide a hot zone along the reactionchamber; a sweep gas inlet adjacent to the first end and configured todirect a sweep gas into the reaction chamber and a sweep gas outletadjacent to the second end and configured to direct an exhaust gas fromthe reaction chamber; a plurality of containers configured in asequentially aligned arrangement within the reactor body, wherein eachcontainer is configured to retain at least one preform, wherein eachcontainer is configured to permit the sweep gas to flow there through,wherein each preform is configured from a mixture of precursor materialsfor a carbothermic reaction, wherein the preform is configured to permitthe sweep gas to flow there through, such that the precursor mixture isreacted in the hot zone to form a ceramic powder product having uniformproperties.

In some embodiments, the reactor body is configured one of vertically orhorizontally.

In some embodiments, the reactor body is configured at an angle, withthe first end at a different height than the second end.

In some embodiments, the reactor further comprises a staging areaconfigured adjacent to and in communication with the first end between areactor inlet and a first seal, wherein the staging area is configuredto accept at least one container, further wherein the staging area isconfigured with a valve such that a pressure differential is introducedthroughout the staging area to remove and/or add gaseous species fromthe staging area.

In some embodiments, the staging area comprises a heat source configuredto preheat the container and the preform.

In some embodiments, the system further comprises: a first seal on thefirst end of the reactor body, wherein the first seal is configured toprovide a sealed reaction chamber adjacent to the first end; and asecond seal on the second end of the reactor body to provide a sealedreaction chamber adjacent to the second end.

In some embodiments, an outer diameter of the container is less than aninner diameter of the reactor body.

In some embodiments, each of the plurality of containers is configuredto support the weight of a plurality of stacked containers equipped withpreforms.

In some embodiments, each of the plurality of containers comprises atleast one end and a sidewall perimetrically surrounding and extendingfrom the end.

In some embodiments, at least one of the ends and the container areconfigured with a mechanical device configured to attach the containersidewall to the end.

In some embodiments, at least one of the container sidewall or thecontainer end is configured with apertures.

In some embodiments, the system is configured for repeated containerinsertion and removal from the reactor body.

In some embodiments, the preform is in a form selected from the groupconsisting of: a sphere, a rod, a plate, a brick, a block, atetrahedron, a torus, a tube, and combinations thereof.

In some embodiments, the preform is selected from the group consistingof: a compacted solid form, an extruded form, a molded form, a castform, and combinations thereof

In some embodiments, the preform is configured to the height of thecontainer.

In some embodiments, the preform is configured in a stacked verticalconfiguration within the container.

In some embodiments, the preform is configured as a rigid body with aporosity configured to permit the sweep gas to permeate through thepreform body.

In one aspect of the instant disclosure, a method for making ceramicpowder, comprises: providing an at least one preform to a reactor, thereactor comprising: a reactor body having a first end and a second end,wherein the reactor body is configured with an inner sidewall extendingfrom the first end to the second end to define a reaction chamber;wherein the reactor body is configured with a heat source to provide ahot zone along the reaction chamber; a plurality of containersconfigured in sequentially aligned arrangement within the reactor body,wherein each container is configured to retain at least one preform,wherein each container is configured to permit the sweep gas to flowthere through, wherein each preform is configured from a mixture ofprecursor materials for a carbothermic reaction, directing a sweep gasfrom the first end through the at least one preform and into the secondend; concomitant with the directing the sweep gas step, carbothermicallyreacting the at least one preform in the reactor body; and forming aceramic powder configured with uniform properties.

In some embodiments, the method further comprises preparing a precursormixture.

In some embodiments, the method further comprises forming the preformfrom the precursor mixture.

In some embodiments, the forming step includes at least one of:compacting the preform mixture; molding the precursor mixture, castingthe precursor mixture, extruding the precursor mixture, and combinationsthereof.

In some embodiments, preparing the precursor mixture further includesone of: (a) forming a wet agglomerate having the reagents therein, or(b) dry processing the reagents with compatible materials and/orbinders.

In some embodiments, the method further comprises processing theprecursor mixture into a preform.

In some embodiments, the processing step includes at least one of:dehydrating the preform, curing the preform, demolding the preform, andcombinations thereof.

In some embodiments, the preform is configured as a body to promoteuniform heat transfer and promote communication of off gases from thepreform.

In some embodiments, the method further comprises: flowing the sweep gas(i) through the preform body; (ii) around the preform body; andcombinations thereof.

In one aspect of the instant disclosure, a system, comprises: a reactorbody having a first end and a second end, wherein the reactor body isconfigured with an inner sidewall extending from the first end to thesecond end to define a reaction chamber; wherein the reactor body isconfigured with a heat source to provide a hot zone along the reactionchamber; a sweep gas inlet adjacent to the first end and configured todirect a sweep gas into the reaction chamber and a sweep gas outletadjacent to the second end and configured to direct an exhaust gas fromthe reaction chamber; a plurality of preforms configured in asequentially aligned arrangement within the reactor body, wherein eachpreform is configured with (1) at least one gas channel configured toextend from the top to the bottom of the preform, parallel to thedirection of gas flow; and (2) a plurality of voids defining a porositywithin the preform body sufficient to permit the sweep gas to flowtherethrough; wherein each preform is configured from a mixture ofprecursor materials for a carbothermic reaction, such that the precursormixture is reacted in the hot zone to form a ceramic powder producthaving uniform properties.

In some embodiments, the gas channel is configured as an area fractionfrom 0.05 area fraction to not greater than 0.8 area fraction of across-sectional area of the reaction chamber.

In some embodiments, the preform is configured from a plurality ofgranules, wherein each granule is configured from the precursor mixture.

In some embodiments, the voids are configured as intra-granule porosityin the preform.

In some embodiments, the intra-granule porosity is configured as an areafraction from 0 to not greater than 0.6 area fraction of across-sectional area of the preform.

In some embodiments, the voids are configured as inter-granule porosityin the preform.

In some embodiments, the inter-granule porosity is configured as an areafraction from 0 to not greater than 0.6 area fraction of across-sectional area of the preform exclusive of the gas channel.

In some embodiments, the voids are configured as a combination ofinter-granule porosity and intra-granule porosity in the preform.

In some embodiments, at least one preform is configured within acontainer, and wherein the container is configured to permit the sweepgas to pass therethrough.

In one aspect of the instant disclosure, a system, comprises: a reactorbody having a first end and a second end, wherein the reactor body isconfigured with an inner sidewall extending from the first end to thesecond end to define a reaction chamber; wherein the reactor body isconfigured with a heat source to provide a hot zone along the reactionchamber; a sweep gas inlet adjacent to the first end and configured todirect a sweep gas into the reaction chamber and a sweep gas outletadjacent to the second end and configured to direct an exhaust gas fromthe reaction chamber; a powder configured from a mixture of precursormaterials for a carbothermic reaction, the powder configured in thereactor chamber to permit sweep gas to flow there through, such that theprecursor mixture is reacted in the hot zone to form a ceramic powderproduct having uniform properties.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 depicts a flow chart for an embodiment of a method for makingceramic powder in accordance with the instant disclosure.

FIG. 2 depicts an embodiment of the system (reactor) in accordance withsome embodiments of the instant disclosure.

FIG. 3 depicts another embodiment of the system (reactor) in accordancewith some embodiments of the instant disclosure.

FIG. 4 depicts cut-away side views of several alternative embodiments ofpreform configurations within a container in accordance with someembodiments of the instant disclosure.

FIG. 5 depicts the top view of the views depicted in FIG. 4 inaccordance with some embodiments of the instant disclosure.

FIG. 6 depicts top plan views of several alternative embodiments ofcontainer end apertures, in accordance with some embodiments of theinstant disclosure.

FIG. 7 depicts a partial cut-away side view of a schematicrepresentation of a preform configured within a container, illustratinga gas channel, inter-granular porosity and intra-granular porosity, inaccordance with various embodiments of the instant disclosure.

To facilitate understanding, identical reference numerals have beenused, where possible, to designate identical elements that are common tothe figures. The figures are not drawn to scale and may be simplifiedfor clarity. It is contemplated that elements and features of oneembodiment may be beneficially incorporated in other embodiments withoutfurther recitation.

DETAILED DESCRIPTION

The present invention will be further explained with reference to theattached drawings, wherein like structures are referred to by likenumerals throughout the several views. The drawings shown are notnecessarily to scale, with emphasis instead generally being placed uponillustrating the principles of the present invention. Further, somefeatures may be exaggerated to show details of particular components

The figures constitute a part of this specification and includeillustrative embodiments of the present invention and illustrate variousobjects and features thereof. Further, the figures are not necessarilyto scale, some features may be exaggerated to show details of particularcomponents. In addition, any measurements, specifications and the likeshown in the figures are intended to be illustrative, and notrestrictive. Therefore, specific structural and functional detailsdisclosed herein are not to be interpreted as limiting, but merely as arepresentative basis for teaching one skilled in the art to variouslyemploy the present invention.

Among those benefits and improvements that have been disclosed, otherobjects and advantages of this invention will become apparent from thefollowing description taken in conjunction with the accompanyingfigures. Detailed embodiments of the present invention are disclosedherein; however, it is to be understood that the disclosed embodimentsare merely illustrative of the invention that may be embodied in variousforms. In addition, each of the examples given in connection with thevarious embodiments of the invention which are intended to beillustrative, and not restrictive.

Throughout the specification and defined embodiments, the followingterms take the meanings explicitly associated herein, unless the contextclearly dictates otherwise. The phrases “in one embodiment” and “in someembodiments” as used herein do not necessarily refer to the sameembodiment(s), though it may. Furthermore, the phrases “in anotherembodiment” and “in some other embodiments” as used herein do notnecessarily refer to a different embodiment, although it may. Thus, asdescribed below, various embodiments of the invention may be readilycombined, without departing from the scope or spirit of the invention.

The term “based on” is not exclusive and allows for being based onadditional factors not described, unless the context clearly dictatesotherwise. In addition, throughout the specification, the meaning of“a,” “an,” and “the” include plural references. The meaning of “in”includes “in” and “on.

FIG. 1 depicts a flow chart for an embodiment of a method 100 for makingceramic powder in accordance with the instant disclosure. In someembodiments, the method 100 may be performed in a suitable reactor, suchas the reactor described below with respect to FIG. 2 and FIG. 3. Insome embodiments, the method 100 begins at 102 by providing an at leastone preform to a suitable reactor. In some embodiments, providing thepreform at 102 includes: (a) forming a precursor mixture, (b) forming apreform from the precursor mixture, and (c) configuring the preform intothe reactor or into a container to be placed within the reactor.

In some embodiments, the precursor mixture is formed by mixing thereagents (e.g. as set out in Table 1), with optional diluents and/orbinders. In some embodiments, forming the precursor mixture furthercomprises one of: (a) forming a wet agglomerate (i.e. a mixture of theraw material reagents and a solvent such as water) having the reagentstherein or (b) dry processing the reagents with compatible materialsand/or binder, including but not limited to polyvinyl alcohol or ethylcellulose, to form an agglomerate.

Referring to Table 1 below, examples of reagents and ceramic powderproducts are provided for three classes of ceramic powder products:borides, carbides, and nitrides. As shown in Table 1, the reagents thatare combinable to form the precursor mixture are depicted in the first1-4 columns, with the ceramic powder product identified to the right ofthe arrow (where the arrow denotes a carbothermic reaction of theprecursor mixture to form the specified ceramic powder product). It isnoted that carbonaceous gases such as carbon monoxide (not shown) arealso produced via carbothermic reduction of the precursor materials.

TABLE 1 Carbothermic Powder Synthesis Reactions Reactants ProductAluminum Oxide Carbon (or Graphite] → Aluminum Carbide Boron Oxide (orCarbon (or Graphite] → Boron Carbide Boric Acid] Chromium Oxide Carbon(or Graphite] → Chromium Carbide Hafnium Oxide Carbon (or Graphite] →Hafnium Carbide Molybdenum Oxide Carbon (or Graphite] → MolybdenumCarbide Niobium Oxide Carbon (or Graphite] → Niobium Carbide SiliconOxide Carbon (or Graphite] → Silicon Carbide Tantalum Oxide Carbon (orGraphite] → Tantalum Carbide Titanium Oxide Carbon (or Graphite] →Titanium Carbide Vanadium Oxide Carbon (or Graphite] → Vanadium CarbideTungsten Oxide Carbon (or Graphite] → Tungsten Carbide Zirconium OxideCarbon (or Graphite] → Zirconium Carbide Aluminum Oxide Boron Oxide (orBoric Acid] Carbon (or Graphite] → Aluminum Boride Chromium Oxide BoronOxide (or Boric Acid] Carbon (or Graphite] → Chromium Boride or ChromiumDiboride Hafnium Oxide Boron Oxide (or Boric Acid] Carbon (or Graphite]→ Hafnium Diboride Niobium Oxide Boron Oxide (or Boric Acid] Carbon (orGraphite] → Niobium Diboride Tantalum Oxide Boron Oxide (or Boric Acid]Carbon (or Graphite] → Tantalum Diboride Titanium Oxide Boron Oxide (orBoric Acid] Carbon (or Graphite] → Titanium Diboride Titanium OxideBoron Oxide (or Boric Acid] Carbon (or Graphite] Ti → TitaniumMonoboride Vanadium Oxide Boron Oxide (or Boric Acid] Carbon (orGraphite] → Vanadium Diboride Zirconium Oxide Boron Oxide (or BoricAcid] Carbon (or Graphite] → Zirconium Diboride Aluminum Oxide BoronOxide (or Boric Acid] Carbon (or Graphite] → Aluminum Boron CarbideAluminum Oxide Nitrogen Carbon (or Graphite] → Aluminum Nitride BoronOxide (or Nitrogen Carbon (or Graphite] → Boron Nitride Boric Acid]Chromium Oxide Nitrogen Carbon (or Graphite] → Chromium Nitride HafniumOxide Nitrogen Carbon (or Graphite] → Hafnium Nitride Molybdenum OxideNitrogen Carbon (or Graphite] → Molybdenum Nitride Niobium OxideNitrogen Carbon (or Graphite] → Niobium Nitride Silicon Oxide NitrogenCarbon (or Graphite] → Silicon Nitride Tantalum Oxide Nitrogen Carbon(or Graphite] → Tantalum Nitride Titanium Oxide Nitrogen Carbon (orGraphite] → Titanium Nitride Vanadium Oxide Nitrogen Carbon (orGraphite] → Vanadium Nitride Tungsten Oxide Nitrogen Carbon (orGraphite] → Tungsten Nitride Zirconium Oxide Nitrogen Carbon (orGraphite] → Zirconium Nitride Aluminum Oxide Nitrogen Carbon (orGraphite] → Aluminum Oxy-Nitride Aluminum Oxide Silicon Oxide Carbon (orGraphite] Nitrogen → Silicon Aluminum Oxy-Nitride

In some embodiments, the amount of the titanium dioxide is 20 weightpercent (wt. %) to 50 wt. % based on a total weight of the precursormixture. In some embodiments, the amount of the titanium dioxide is 25wt. % to 50 wt. % based on a total weight of the precursor mixture. Insome embodiments, the amount of the titanium dioxide is 30 wt. % to 50wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of the titanium dioxide is 35 wt. % to 50 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of the titanium dioxide is 40 wt. % to 50 wt. % based on atotal weight of the precursor mixture. In some embodiments, the amountof the titanium dioxide is 45 wt. % to 50 wt. % based on a total weightof the precursor mixture.

In some embodiments, the amount of the titanium dioxide is 20 wt. % to45 wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of the titanium dioxide is 20 wt. % to 40 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of the titanium dioxide is 20 wt. % to 35 wt. % based on atotal weight of the precursor mixture. In some embodiments, the amountof the titanium dioxide is 20 wt. % to 30 wt. % based on a total weightof the precursor mixture. In some embodiments, the amount of thetitanium dioxide is 20 wt. % to 25 wt. % based on a total weight of theprecursor mixture.

In some embodiments, the amount of the titanium dioxide is 25 wt. % to45 wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of the titanium dioxide is 30 wt. % to 40 wt. %based on a total weight of the precursor mixture.

In some embodiments, the amount of the carbon source is 10 wt. % to 35wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of the carbon source is 15 wt. % to 35 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of the carbon source is 20 wt. % to 35 wt. % based on a totalweight of the precursor mixture. In some embodiments, the amount of thecarbon source is 25 wt. % to 35 wt. % based on a total weight of theprecursor mixture. In some embodiments, the amount of the carbon sourceis 30 wt. % to 35 wt. % based on a total weight of the precursormixture.

In some embodiments, the amount of the carbon source is 10 wt. % to 30wt .% based on a total weight of the precursor mixture. In someembodiments, the amount of the carbon source is 10 wt. % to 25 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of the carbon source is 10 wt. % to 20 wt. % based on a totalweight of the precursor mixture. In some embodiments, the amount of thecarbon source is 10 wt. % to 15 wt. % based on a total weight of theprecursor mixture.

In some embodiments, the amount of the carbon source is 15 wt. % to 30wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of the carbon source is 15 wt. % to 25 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of the carbon source is 20 wt. % to 25 wt. % based on a totalweight of the precursor mixture.

In some embodiments, the amount of boric acid is 30 wt. % to 70 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of boric acid is 30 wt. % to 65 wt. % based on a total weightof the precursor mixture. In some embodiments, the amount of boric acidis 30 wt. % to 60 wt. % based on a total weight of the precursormixture. In some embodiments, the amount of boric acid is 30 wt. % to 55wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of boric acid is 30 wt. % to 50 wt. % based on atotal weight of the precursor mixture. In some embodiments, the amountof boric acid is 30 wt. % to 45 wt. % based on a total weight of theprecursor mixture. In some embodiments, the amount of boric acid is 30wt. % to 40 wt. % based on a total weight of the precursor mixture. Insome embodiments, the amount of boric acid is 30 wt. % to 35 wt. % basedon a total weight of the precursor mixture.

In some embodiments, the amount of boric acid is 35 wt. % to 70 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of boric acid is 40 wt. % to 70 wt. % based on a total weightof the precursor mixture. In some embodiments, the amount of boric acidis 45 wt. % to 70 wt. % based on a total weight of the precursormixture. In some embodiments, the amount of boric acid is 50 wt. % to 70wt. % based on a total weight of the precursor mixture. In someembodiments, the amount of boric acid is 55 wt. % to 70 wt. % based on atotal weight of the precursor mixture. In some embodiments, the amountof boric acid is 60 wt. % to 70 wt. % based on a total weight of theprecursor mixture. In some embodiments, the amount of boric acid is 65wt. % to 70 wt. % based on a total weight of the precursor mixture.

In some embodiments, the amount of boric acid is 35 wt. % to 65 wt. %based on a total weight of the precursor mixture. In some embodiments,the amount of boric acid is 40 wt. % to 60 wt. % based on a total weightof the precursor mixture. In some embodiments, the amount of boric acidis 45 wt. % to 55 wt. % based on a total weight of the precursormixture.

In some embodiments, the precursor mixture is formed into a preform. Asused herein, “preform” means a shaped mixture of precursor materialsconfigured to enable/permit gas to flow through the preform.

In one non-limiting example, forming of the precursor mixture into atleast one preform includes adding the pliable, hydrated precursormixture into a mold, compacting the mixture in the mold (e.g. in thetarget shape of the preform), followed by dehydrating the mixture atelevated temperatures (e.g. at sufficient temperature and time to (1)drive off water from the precursor mixture and (2) configure the preformin a hardened, stable shape).

In one non-limiting example, forming of the precursor mixture into atleast one preform includes casting (pouring and/or directing) theflowable, hydrated precursor mixture into a mold, and processing theprecursor mixture into the preform by (1) removing excess water from theprecursor mixture to configure the preform from the as-cast shape.

In one non-limiting example, forming of the precursor mixture into atleast one preform includes directing the pliable, hydrated precursormixture into an extrusion press, and extruding the precursor mixturethrough an extrusion die in order to form an extrudate, followed byprocessing the extrudate to remove any excess water and provide apreform from the extruded precursor mixture.

In some embodiments, the preform is removed from the mold or castsupport prior to being directed into the reactor body.

In some embodiments, the compacting step is conducted with a compactiontool. In some embodiments, the dehydration step is conducted using air(or other gas) or heat (e.g. a furnace).

In some embodiments the preform is configured with (a) at least one gaschannel and (b) macro-porosity in at least a portion of the preform body(e.g. where macro-porosity refers to sufficiently sized voids to permitgas to permeate through the preform).

In some embodiments, the preform is configured to take up 0.2 to 0.95area fraction when viewing a cross-sectional area across the reactionchamber. In some embodiments, the preform is configured to take up: 0.5to 0.95 area fraction; 0.55 to 0.95 area fraction; 0.6 to 0.95 areafraction; 0.65 to 0.95 area fraction; 0.7 to 0.95 area fraction; 0.75 to0.95 area fraction; 0.8 to 0.95 area fraction; 0.85 to 0.95 areafraction; or 0.9 to 0.95 area fraction, when viewing a cross-sectionalarea across the reaction chamber.

In some embodiments, the preform is configured to take up: 0.2 to 0.90area fraction; 0.2 to 0.85 area fraction; 0.2 to 0.80 area fraction; 0.2to 0.75 area fraction; 0.2 to 0.70 area fraction; 0.2 to 0.65 areafraction; 0.2 to 0.60 area fraction; 0.2 to 0.55 area fraction; 0.2 to0.50 area fraction; or 0.2 to 0.40 area fraction, when viewing across-sectional area across the reaction chamber.

In some embodiments, the preform is configured to take up 0.2 areafraction to not greater than 0.95 area fraction of a cross-sectionalarea taken across the reaction chamber. In some embodiments, the preformis configured to take up 0.6 area fraction to not greater than 0.95 areafraction of a cross-sectional area taken across the reaction chamber. Insome embodiments, the preform is configured to take up 0.75 areafraction to not greater than 0.95 area fraction of a cross-sectionalarea taken across the reaction chamber.

In some embodiments, the preform is configured from a plurality ofgranules. In some embodiments, the preform is configured withinter-granule porosity, which is measured between granules of a singlepreform.

In some embodiments, the inter-granule porosity is configured to take up0 to 0.6 area fraction when viewing a cross-sectional area across thepreform exclusive of gas channels. In some embodiments, theinter-granule porosity is configured to take up: 0.1 to 0.6 areafraction; 0.2 to 0.6 area fraction; 0.3 area to 0.6 fraction; 0.4 to 0.6area fraction; or 0.5 to 0.6 area fraction, when viewing across-sectional area across the preform, exclusive of gas channels.

In some embodiments, the inter-granule porosity is configured to takeup: 0 to 0.5 area fraction; 0 to 0.4 area fraction; 0 to 0.3 areafraction; 0 to 0.2 area fraction; 0 to 0.1 area fraction, when viewing across-sectional area across the preform, exclusive of gas channels.

In some embodiments, the inter-granule porosity is configured to take up0 area fraction to not greater than 0.6 area fraction of across-sectional area taken across the preform, exclusive of gaschannels. In some embodiments, the preform is configured to take up 0.2area fraction to not greater than 0.6 area fraction of a cross-sectionalarea taken across the preform, exclusive of gas channels. In someembodiments, the preform is configured to take up 0.3 area fraction tonot greater than 0.6 area fraction of a cross-sectional area takenacross the preform, exclusive of gas channels.

In some embodiments, the preform is configured with intra-granuleporosity, which is measured within a single granule (e.g. porositybetween precursor mixture/reagents).

In some embodiments, there is inter-granule porosity and nointra-granular porosity (0 area fraction). In some embodiments, there isintra-granule porosity and no inter-granule porosity.

In some embodiments, the intra-granule porosity is configured to take upnot greater than 0 area fraction; not greater than 0.05 area fraction;not greater than 0.1 area fraction; not greater than 0.2 area fraction;not greater than 0.3 area fraction; not greater than 0.4 area fraction;not greater than 0.5 area fraction; or not greater than 0.6 areafraction, when viewing a cross-sectional area across the preform.

In some embodiments, the intra-granule porosity is configured to take up0 area fraction to not greater than 0.6 area fraction of across-sectional area taken across the preform. In some embodiments, theintra-granule porosity is configured to take up 0 area fraction to notgreater than 0.5 area fraction of a cross-sectional area taken acrossthe preform. In some embodiments, the intra-granule porosity isconfigured to take up 0 area fraction to not greater than 0.4 areafraction of a cross-sectional area taken across the preform. In someembodiments, the intra-granule porosity is configured to take up 0 areafraction to not greater than 0.3 area fraction of a cross-sectional areataken across the preform.

In some embodiments, the preform is configured with at least one gaschannel.

As used herein, “gas channel” refers to the open space/volume that isnot taken up by the preform (and/or the container, if a container isutilized), in the cross-sectional area of the reaction chamber. In someembodiments, the gas channel is configured in a direction parallel tothe gas flow through the preform body.

In some embodiments, the gas channel is configured to take up 0.05 to0.8 area fraction when viewing a cross-sectional area across thereaction chamber. In some embodiments, the gas channel is configured totake up: 0.1 to 0.8 area fraction; 0.1 to 0.7 area fraction; 0.1 to 0.6area fraction; 0.1 to 0.5 area fraction; 0.1 to 0.4 area fraction; 0.1to 0.3 area fraction; or 0.1 to 0.2 area fraction, when viewing across-sectional area across the reaction chamber.

In some embodiments, the gas channel is configured to take up: 0.1 to0.8 area fraction; 0.2 to 0.8 area fraction; 0.3 to 0.8 area fraction;0.4 to 0.8 area fraction; 0.5 to 0.8 area fraction; 0.6 to 0.8 areafraction; or 0.7 to 0.8 area fraction, when viewing a cross-sectionalarea across the reaction chamber.

In some embodiments, the gas channel is configured to take up from atleast 0.05 area fraction to not greater than 0.8 area fraction, of across-sectional area taken across the reaction chamber. In someembodiments, the gas channel is configured to take up at least 0.1 areafraction to not greater than 0.8 area fraction, of a cross-sectionalarea taken across the reaction chamber. In some embodiments, the gaschannel is configured to take up from at least 0.2 area fraction to notgreater than 0.8 area fraction, of a cross-sectional area taken acrossthe reaction chamber. In some embodiments, the gas channel is configuredto take up from at least 0.3 area fraction to not greater than 0.8 areafraction, of a cross-sectional area taken across the reaction chamber.

In some embodiments, when the preform is sized such that one or morepreforms fit into a container, one or more gas channels are configuredfrom the container (e.g. a mesh wall defining a vertical gas channelwithin the plurality of preforms, see, e.g. FIG. 5H).

In some embodiments, the diameter of the preform is 2 inches to 48inches. In some embodiments, the diameter of the preform is 2 inches to42 inches. In some embodiments, the diameter of the preform is 2 inchesto 36 inches. In some embodiments, the diameter of the preform is 2inches to 30 inches. In some embodiments, the diameter of the preform is2 inches to 24 inches. In some embodiments, the diameter of the preformis 2 inches to 18 inches. In some embodiments, the diameter of thepreform is 2 inches to 12 inches. In some embodiments, the diameter ofthe preform is 2 inches to 10 inches. In some embodiments, the diameterof the preform is 2 inches to 8 inches. In some embodiments, thediameter of the preform is 2 inches to 6 inches. In some embodiments,the diameter of the preform is 2 inches to 4 inches.

In some embodiments, the diameter of the preform is 4 inches to 48inches. In some embodiments, the diameter of the preform is 6 inches to48 inches. In some embodiments, the diameter of the preform is 8 inchesto 48 inches. In some embodiments, the diameter of the preform is 10inches to 48 inches. In some embodiments, the diameter of the preform is12 inches to 48 inches. In some embodiments, the diameter of the preformis 18 inches to 48 inches. In some embodiments, the diameter of thepreform is 24 inches to 48 inches. In some embodiments, the diameter ofthe preform is 30 inches to 48 inches. In some embodiments, the diameterof the preform is 36 inches to 48 inches. In some embodiments, thediameter of the preform is 42 inches to 48 inches.

In some embodiments, the diameter of the preform is 4 inches to 6inches. In some embodiments, the diameter of the preform is 4 inches to8 inches. In some embodiments, the diameter of the preform is 4 inchesto 10 inches. In some embodiments, the diameter of the preform is 6inches to 12 inches. In some embodiments, the diameter of the preform is12 inches to 24 inches. In some embodiments, the diameter of the preformis 24 inches to 36 inches. In some embodiments, the diameter of thepreform is 36 inches to 48 inches.

In some embodiments, the “diameter of the at least one opening” meanseither the diameter of each opening or the sum of the diameters of allthe openings in the preform. In some embodiments, the diameter of the atleast one opening is 0 inches to 46 inches. In some embodiments, thediameter of the at least one opening is ¼ inch to 46 inches. In someembodiments, the diameter of the at least one opening is 2 inches to 46inches. In some embodiments, the diameter of the at least one opening is3 inches to 46 inches. In some embodiments, the diameter of the at leastone opening is 4 inches to 46 inches. In some embodiments, the diameterof the at least one opening is 5 inches to 46 inches. In someembodiments, the diameter of the at least one opening is 8 inches to 46inches. In some embodiments, the diameter of the at least one opening is12 inches to 46 inches. In some embodiments, the diameter of the atleast one opening is 16 inches to 46 inches. In some embodiments, thediameter of the at least one opening is 20 inches to 46 inches. In someembodiments, the diameter of the at least one opening is 24 inches to 46inches. In some embodiments, the diameter of the at least one opening is28 inches to 46 inches. In some embodiments, the diameter of the atleast one opening is 32 inches to 46 inches. In some embodiments, thediameter of the at least one opening is 36 inches to 46 inches. In someembodiments, the diameter of the at least one opening is 40 inches to 46inches.

In some embodiments, the diameter of the at least one opening is 0inches to 42 inches. In some embodiments, the diameter of the at leastone opening is 0 inches to 36 inches. In some embodiments, the diameterof the at least one opening is 0 inches to 32 inches. In someembodiments, the diameter of the at least one opening is 0 inches to 28inches. In some embodiments, the diameter of the at least one opening is0 inches to 24 inches. In some embodiments, the diameter of the at leastone opening is 0 inches to 20 inches. In some embodiments, the diameterof the at least one opening is 0 inches to 16 inches. In someembodiments, the diameter of the at least one opening is 0 inches to 12inches. In some embodiments, the diameter of the at least one opening is0 inches to 10 inches. In some embodiments, the diameter of the at leastone opening is 0 inches to 8 inches. In some embodiments, the diameterof the at least one opening is 0 inches to 6 inches. In someembodiments, the diameter of the at least one opening is 0 inches to 4inches.

In some embodiments, the diameter of the at least one opening is 1inches to 3 inches. In some embodiments, the diameter of the at leastone opening is 3 inches to 8 inches. In some embodiments, the diameterof the at least one opening is 6 inches to 24 inches. In someembodiments, the diameter of the at least one opening is 10 inches to 30inches. In some embodiments, the diameter of the at least one opening is12 inches to 36 inches.

In some embodiments, the diameter of the at least one opening is based,at least in part, on achieving substantially uniform heating throughoutthe preform (i.e. throughout the volume of the preform).

In some embodiments, the height of the preform is 2 inches to 48 inches.In some embodiments, the height of the preform is 4 inches to 48 inches.In some embodiments, the height of the preform is 6 inches to 48 inches.In some embodiments, the height of the preform is 8 inches to 48 inches.In some embodiments, the height of the preform is 12 inches to 48inches. In some embodiments, the height of the preform is 16 inches to48 inches. In some embodiments, the height of the preform is 20 inchesto 48 inches. In some embodiments, the height of the preform is 24inches to 48 inches. In some embodiments, the height of the preform is28 inches to 48 inches. In some embodiments, the height of the preformis 32 inches to 48 inches. In some embodiments, the height of thepreform is 36 inches to 48 inches. In some embodiments, the height ofthe preform is 40 inches to 48 inches. In some embodiments, the heightof the preform is 44 inches to 48 inches.

In some embodiments, the height of the preform is 2 inches to 44 inches.In some embodiments, the height of the preform is 2 inches to 40 inches.In some embodiments, the height of the preform is 2 inches to 36 inches.In some embodiments, the height of the preform is 2 inches to 32 inches.In some embodiments, the height of the preform is 2 inches to 28 inches.In some embodiments, the height of the preform is 2 inches to 24 inches.In some embodiments, the height of the preform is 2 inches to 20 inches.In some embodiments, the height of the preform is 2 inches to 16 inches.In some embodiments, the height of the preform is 2 inches to 12 inches.In some embodiments, the height of the preform is 2 inches to 8 inches.In some embodiments, the height of the preform is 2 inches to 6 inches.In some embodiments, the height of the preform is 2 inches to 4 inches.

In some embodiments, the height of the preform is 4 inches to 8 inches.In some embodiments, the height of the preform is 8 inches to 16 inches.In some embodiments, the height of the preform is 12 inches to 24inches. In some embodiments, the height of the preform is 8 inches to 42inches. In some embodiments, the height of the preform is 4 inches to 8inches. In some embodiments, the height of the preform is 16 inches to28 inches. In some embodiments, the height of the preform is 6 inches to24 inches.

Next, at 104, the method 100 comprises directing a sweep gas from afirst end of the reactor, through the at least one preform, and into thesecond end of the reactor.

In some embodiments, when the ceramic powder is a carbide, the sweep gasis selected from the group of: argon or any other noble gas, carbonmonoxide, carbon dioxide, and/or combinations thereof.

In some embodiments, when the ceramic powder is a nitride, the sweep gasis nitrogen or combinations of nitrogen and noble gas. In someembodiments, when the ceramic powder is a boride, the sweep gas is argonor any other noble gas.

In some embodiments, the flow rate of the sweep gas is sufficient toremove or reduce the concentration of the reaction byproducts in thereactor and/or sufficient to manage atmospheric chemistry in thereactor. In some embodiments, the sweep gas flow rate is based, at leastin part, on the reactor geometry, the desired ceramic powder, thetemperature profile within the reactor and/or other process conditionsrelated to the powder production.

In some embodiments, the sufficient time is dependent on type ofreagents and powder and the sufficient temperature. In some embodiments,the sufficient time is 0.5 hour to 12 hours. In some embodiments, thesufficient time is 0.5 hour to 11 hours. In some embodiments, thesufficient time is 0.5 hour to 10 hours. In some embodiments, thesufficient time is 0.5 hour to 9 hours. In some embodiments, thesufficient time is 0.5 hour to 8 hours. In some embodiments, thesufficient time is 0.5 hour to 7 hours. In some embodiments, thesufficient time is 0.5 hour to 6 hours. In some embodiments, thesufficient time is 0.5 hour to 5 hours. In some embodiments, thesufficient time is 0.5 hour to 4 hours. In some embodiments, thesufficient time is 0.5 hour to 3 hours. In some embodiments, thesufficient time is 0.5 hour to 2 hours. In some embodiments, thesufficient time is 0.5 hour to 1 hours.

In some embodiments, the sufficient time is 1 hour to 12 hours. In someembodiments, the sufficient time is 2 hours to 12 hours. In someembodiments, the sufficient time is 3 hours to 12 hours. In someembodiments, the sufficient time is 4 hours to 12 hours. In someembodiments, the sufficient time is 5 hours to 12 hours. In someembodiments, the sufficient time is 6 hours to 12 hours. In someembodiments, the sufficient time is 7 hours to 12 hours. In someembodiments, the sufficient time is 8 hours to 12 hours. In someembodiments, the sufficient time is 9 hours to 12 hours. In someembodiments, the sufficient time is 10 hours to 12 hours. In someembodiments, the sufficient time is 11 hours to 12 hours.

In some embodiments, the sufficient time is 1 hour to 8 hours. In someembodiments, the sufficient time is 1 hour to 6 hours. In someembodiments, the sufficient time is 1 hour to 4 hours. In someembodiments, the sufficient time is 1 hour to 2 hours. In someembodiments, the sufficient time is 2 hour to 11 hours. In someembodiments, the sufficient time is 3 hour to 10 hours. In someembodiments, the sufficient time is 4 hour to 9 hours. In someembodiments, the sufficient time is 5 hour to 8 hours. In someembodiments, the sufficient time is 6 hour to 7 hours.

In some embodiments, the powder is titanium diboride and the sufficienttime is 1 hour to 6 hours. In some embodiments, the powder is titaniumdiboride and the sufficient time is 1 hour to 5 hours. In someembodiments, the powder is titanium diboride and the sufficient time is1 hour to 4 hours. In some embodiments, the powder is titanium diborideand the sufficient time is 1 hour to 3 hours. In some embodiments, thepowder is titanium diboride and the sufficient time is 1 hour to 2hours. In some embodiments, the powder is titanium diboride and thesufficient time is 2 hour to 6 hours. In some embodiments, the powder istitanium diboride and the sufficient time is 3 hour to 6 hours. In someembodiments, the powder is titanium diboride and the sufficient time is4 hour to 6 hours. In some embodiments, the powder is titanium diborideand the sufficient time is 5 hour to 6 hours.

In some embodiments, the sufficient temperature and sufficient time arecombinations of the temperatures and times detailed above.

Next, at 106, the method 100 comprises carbothermically reacting the atleast one preform within the reactor body, concomitant with directingthe sweep gas. In some embodiments, carbothermically reacting the atleast one preform within the reactor body, concomitant with directingthe sweep gas comprises: directing the at least one preform (e.g.housed/retained in a container) through the reactor body, and heatingthe at least one preform (comprising a precursor mixture) to asufficient temperature for a sufficient time to form a ceramic powderproduct via carbothermic reaction of the reagents in the precursormixture. Non-limiting examples of carbothermic reactions forming ceramicpowders are shown in Table 1

As used herein, the term “carbothermic reaction” means a reaction thatincludes the reduction of substances using carbon as the reducing agentat elevated temperatures typically ranging from about 500 to about 2,500degrees Celsius. In some embodiments, the sufficient temperature (tocarbothermically react the precursor mixture) is dependent on the typeof reagents and powder utilized to form the precursor mixture.

Next, at 108, the method 100 comprises forming a ceramic powder productconfigured with uniform and/or consistent properties. In someembodiments, the method 100 continuously produces the ceramic powderproducts in the heated reactor, including as non-limiting examples:borides, nitrides, and/or carbides. In some embodiments, the ceramicpowder is any powder described herein. In some embodiments, the ceramicpowder product includes, but is not limited to, titanium diboride, boroncarbide, boron nitride, aluminum nitride, silicon aluminum nitride,zirconium diboride, aluminum nitride, silicon aluminum oxy-nitride,titanium carbide, silicon carbide, titanium nitride, and aluminumcarbide.

As used herein, “consistent properties” means: that preforms that aredirected through the carbothermic reactor (e.g. at different timesand/or in different containers) exhibit properties including but notlimited to particle size distribution, surface area, chemicalcomposition, and particle shape, that are measurably indistinguishableand/or compatible with the specification for the final ceramic powderproduct (e.g. where properties are analytically determined and/orevaluated).

As used herein, “uniform properties” means: that the properties (e.g.qualitatively measured and/or quantitatively measured) are generallyunchanging and/or invariable in form or character (e.g. in comparingceramic powder product recovered from one preform to ceramic powderproduct recovered from another preform).

In some embodiments, the method further comprises removing the ceramicpowder product from the reactor. In some embodiments, the ceramic powderproduct is removed from the reactor in a receiving unit having an inertatmosphere so as to maintain an inert environment in the verticalreactor.

FIG. 2 depicts an embodiment of the system (reactor) in accordance withthe instant disclosure. Referring to FIG. 2, a system 10 is depicted,including a reactor body 12 configured with a staging area 42, areceiving unit 60, gas sweep 28 (gas inlet 26 and gas outlet 30) and asealed configuration across the reactor body (e.g. seal 46 and seal 52).In some embodiments, the reactor body 12 is vertical, horizontal, or anyangle between 0 and 90 degrees. In some embodiments as shown in FIG. 2and FIG. 3, the reactor body 12 is vertical. In some embodiments, thereactor body is coupled to a heat source 22 to provide a hot zone 24along the reaction chamber.

In some embodiments, a cross-section of the reactor body is in a circle,square, rectangular, pentagon, hexagon, or any other suitable shape. Insome embodiments, the reactor is graphite, silicon carbide, boronnitride, alumina, molybdenum, tungsten, or other refractory materialsthat are compatible with the reagents and/or byproducts.

As shown in FIGS. 2 and 3, preforms 36 (e.g. retained in at least onecontainer 34) are directed into the staging area 42. The staging area 2is enclosed/sealed and equipped with a valve 48. Valve 48 is configuredfor inserting a positive pressure (e.g. gas purge of staging area 42 andpreforms 36). Valve 48 is also configured to insert a negative pressure(e.g. pull a vacuum through the staging area 42 and or preforms 36).Staging area 42 is also equipped with a heat source 50, such that thepreforms 36 and container(s) 34 can be preheated prior to entering thereactor body.

After the preform 36 travels through the staging area 42, the preform 36crosses the seal 46 adjacent to the first end 14 of the reactor body andis introduced into the reaction chamber 20. The preform 36 and/orcontainer 34 is sufficiently sized such that it is retained in closeproximity with the inner sidewall 18 of the reactor 12 such that theouter diameter of the container 34 is less than the diameter of theinner sidewall 18. The preform 36 (e.g. and container) is heated in thepreheat zone 44, after which the preform 36 is directed into the hotzone 24 of the reaction chamber 20. In the hot zone 24, the temperatureis sufficient to promote carbothermic reaction of the precursor material38, provided the preforms 36 are retained in the hot zone 24 for asufficient time.

Within the reaction chamber 20, the containers 34 containing at leastone preform 36 are aligned with each other such that the containers aresequentially configured throughout the reaction chamber. The ends ofcontainers 34 are coincidental to one another such that the containers34 are arranged in a position relative to one another such that eachindividual container is a component 70 of a sequentially configuredcontainer assembly in the reaction chamber 20. Thus, as depicted inFIGS. 2 and 3, the preform (e.g. and container) are directed through thesystem 10 (e.g. from the staging area 42 to the hot zone 24 of thereaction chamber 20 and finally to the receiving unit 60) in a meteredand/or indexed fashion. In some embodiments, the system is configuredsuch that each preform is exposed to an identical reaction profile (e.g.gas flow rate, thermal profile in the reaction chamber) such that theceramic powder product is configured with uniform and/or consistentproperties.

As depicted in FIG. 2, the direction of the sweep gas 28 is countercurrent to the direction of movement of the preforms 36 in the reactionchamber 20. As depicted in FIG. 3, the direction of the sweep gas 28 isco-current to the direction of movement of the preforms 36 in thereaction chamber 20.

As the preforms reach the end of the reaction chamber 20, the preforms36 are directed through a seal 52 (configured adjacent to the second end16) and directed out of the reactor to the receiving unit 60. As thepreforms 36 are adjacent to the second end 16 and/or seal 52, thecarbothermic reaction of precursor materials is complete, yielding theceramic powder product 40. In some embodiments, the ceramic powderproduct 40 is generally retained in the preform 36, such that oncereceived in the receiving unit 60, a deagglomeration step or breaking upof the preform 36 shape may be utilized to yield a ceramic powderproduct 40 (e.g. deagglomerated powder).

In some embodiments, the reactor includes a lid configured to directprocess gas flow into or out of the reactor. In some embodiments, thelid is configured with a plurality of openings to allow for control ofthe gas flow rate into and out of the reactor.

In some embodiments, the inner diameter and the height (or length) ofthe reactor body are selected based on the diameter, thickness andnumber of preforms to be positioned in the reactor. In some embodiments,the inner diameter of the reactor is sufficiently greater than thediameter of the preform so as to allow flow of the inert gas between thereactor and the preform and/or to reduce or eliminate contact of thepreform with a sidewall of the reactor. In some embodiments, the reactorincludes a sufficient number of preforms (e.g. configured in containers)to fill the reactor based on the height (or length if horizontal) of thereactor. In some embodiments, the number of preforms in the reactors isthe height (or length if horizontal) of the reactor divided by theheight of the preform.

In some embodiments, the preforms are stacked in, added to and/orremoved from the reactor at a controlled rate by any suitable mechanicaldevices, configurations, components, and/or related means. In someembodiments, the controlled rate of stacking, adding and removing thepreforms is based, at least in part, on the reaction rate of thereagents in the preform. In some embodiments, the unreacted preforms andthe reacted preforms are added to and removed from the reactor through aseal (e.g. configured with a sweep gas) so that the process atmosphereis maintained within the reactor.

FIG. 4 depicts cut-away side views of several alternative embodiments ofpreform configurations within a container in accordance with the instantdisclosure. FIG. 5 depicts the top view of the views depicted in FIG. 4.

More specifically referring to FIGS. 4 and 5, A depicts a containerconfigured to retain a single preform (showing two containers eachconfigured with an end and a single preform retained therein, where thetwo containers are configured in a vertically stacked configuration); Bdepicts multiple preforms stacked vertically within one container withno spacer or plate between the two preforms (one end at the lower regionof the container); C depicts preforms stacked on top of each otherwithin a single container, where the container was configured with aspacer in the form of a plenum/perforated plate (e.g. configured topermit gases and/or heat to communicate through the container vaporspace and/or out the ends); where in contrast to A-C, D depicts adifferent configuration of the same preform shape within a container,D-H depict different forms/shapes of preforms.

More specifically, D depicts a plurality of rods retained in a generallyparallel configuration with sufficient vapor space in the container topromote communication of off gases from the rods and through thecontainer end); E depicts a plurality of vertically and generallyparallel stacked forms (e.g. brick preforms) in the container; F depictsa plurality of sphere preforms retained in the container; G depictsheterogeneously sized preforms in the container (spheres havingdifferent sized diameters: small, medium, and large); while H depicts aplurality of preforms that are each a compacted solid material.

In some embodiments, the preforms shown in FIGS. 5C and 5H can be formedvia extrusion to produce preforms having continuous straight gaschannels in the vertical direction and uniform geometry in the x-yplane.

FIG. 6 depicts top plan views of several alternative embodiments ofcontainer end 54 apertures 58, in accordance with the instantdisclosure. FIG. 6A depicts a large centrally positioned aperture 58,with a concentric circle of smaller apertures 58 surrounding the centralaperture 58 on the container end 54. FIG. 6B depicts multiple rows ofapertures 54 (e.g. two rows of concentrically configured apertures 58)in the container end 54. FIGS. 6C and 6E both show apertures configuredas a fence (6C) or mesh (6E) configuration, such that more open space(aperture area) than closed space (end area) is taken up by end 54. FIG.6D depicts apertures 58 that are symmetrically configured/equidistantlyconfigured on the container end 54. As depicted in the variousembodiments of FIG. 6, multiple alternative embodiments for aperturescan be utilized in accordance with the present disclosure, such that theresulting container is configured to promote uniform gastransfer/movement into and out of the corresponding container and/orpreform(s) retained therein, as the containers and preform(s) travelthrough the reaction chamber 20).

FIG. 7 depicts a partial cut-away side view of a schematicrepresentation of a preform 36 configured within a container 34. Asdepicted in FIG. 7, there is a gas channel 66 positioned between thesidewall 56 of the container 34 and the preform 36. Also, the preform 36is depicted as a body configured from a plurality of granules 72. Thepreform 36 has voids 68 defined as a combination of inter-granularporosity 74 and intra-granular porosity 76. Also, examples of ranges ofthe area fractions of various components of the preform are provided inthe table included in FIG. 7.

In some embodiments, the ceramic powders detailed herein may be used formultiple applications. In some embodiments, the ceramic powders arespecifically tailored to be processed via ceramics processing techniquesin order to form ceramic products (wherein the ceramic products aretailored for their application, based on the consistent and/or uniformproperties of the ceramic powder product).

While a number of embodiments of the present invention have beendescribed, it is understood that these embodiments are illustrativeonly, and not restrictive, and that many modifications may becomeapparent to those of ordinary skill in the art. Further still, thevarious steps may be carried out in any desired order (and any desiredsteps may be added and/or any desired steps may be eliminated).

REFERENCE NUMBERS

-   System 10-   Reactor body 12-   First end 14-   Second end 16-   Inner sidewall 18-   Reaction chamber 20-   Heat source 22-   Hot zone 24-   Sweep gas inlet 26-   Sweep gas 28-   Sweep gas outlet 30-   Exhaust gas 32-   Container 34-   Preform 36-   Precursor materials 38-   Ceramic powder product 40-   Staging area 42-   Preheat zone 44-   First seal 46-   Valve 48-   Heat source 50-   Second seal 52-   At least one end (of container) 54-   Sidewall (of container) 56-   Apertures (on end or container sidewall) 58-   Receiving unit 60-   Vapor space in container (e.g. defined as the space between the    preform(s) and the container end and/or sidewalls) 62-   Separator plate (e.g. plenum plate, e.g. configured as a spacer for    preform(s) within a single container) 64-   Gas channel/at least one opening (e.g. in the preform) 66-   Porosity/voids (in preform) 68 (includes e.g. inter-granule and    intra-granule, when preform is configured from granules)-   Component (e.g. includes container and at least one preform, where    the components are configurable in a container assembly    (sequentially configured, aligned plurality of containers)-   Granule 72-   Inter-granule porosity 74-   Intra-granule porosity 76 (e.g. or intra-preform porosity, if    utilizing compacted solid preform, cast preform and/or extrudate    preform)

1-36. (canceled)
 37. A method for carbothermically producing a ceramicpowder, the method comprising: a) preheating at least one container in astaging zone, wherein the at least one container comprises at least onepreform, wherein the preform comprises carbon; b) moving the at leastone container into a reactor body, wherein the reactor body comprises areaction zone; c) carbothermically reacting the at least one preform inthe reaction zone thereby producing a ceramic powder, wherein thecarbothermically reacting comprises reducing, via the carbon of thepreform, a metal compound of the preform to a metal carbide, a metalboride, or a metal nitride; and d) moving the at least one containerfrom the reactor body to a receiving zone.
 38. The method of claim 37,comprising flowing, during at least the carbothermically reacting step,a sweep gas into the at least one container.
 39. The method of claim 38,wherein the at least one preform comprises a porosity, wherein theflowing comprises flowing the sweep gas through at least one pore of theat least one preform.
 40. The method of claim 37, wherein thecarbothermically reacting step comprises a reaction time, wherein thereaction time is from 0.5 to 12 hours.
 41. The method of claim 37,wherein the ceramic powder is selected from the group consisting oftitanium diboride, boron carbide, boron nitride, aluminum nitride,silicon aluminum nitride, zirconium diboride, silicon aluminumoxy-nitride, titanium carbide, silicon carbide, titanium nitride,aluminum carbide, and combinations thereof.
 42. A system comprising: a)a staging area, wherein the staging area comprises at least onecontainer, wherein the at least one container comprises at least onepreform, and wherein the at least one preform comprises carbon and atleast one of a metal oxide and boric acid; b) a reactor body adapted toreceive the at least one container from the staging area; c) a receivingunit adapted to receive the at least one container from the reactorbody; d) a heat source coupled to the reactor body, wherein the heatsource is configured to produce carbothermic reaction temperaturesrelative to the at least one preform.
 43. The system of claim 42,wherein the reactor body comprises a sweep gas inlet and a sweep gasoutlet.
 44. The system of claim 42, wherein at least the reactor bodycomprises a plurality of containers in sequential alignment.
 45. Thesystem of claim 42, wherein the staging area comprises a one-way valveor a two-way valve.
 46. The system of claim 42, wherein the reactor bodycomprises a first seal, wherein the first seal is in fluid communicationwith the staging area.
 47. The system of claim 42, wherein the reactorbody comprises a second seal, wherein the second seal is in fluidcommunication with the receiving unit.
 48. The system of claim 42,wherein the at least one container comprises a sidewall, wherein thesidewall comprises a mechanical device adapted to attach the at leastone container to the reactor body.
 49. The system of claim 42, whereinthe at least one container comprises at least one aperture.
 50. Thesystem of claim 42, wherein the reactor body comprises a reactionchamber, wherein the at least one preform comprises a gas channel, andwherein the gas channel comprises an area fraction of from 0.05 to 0.8of a cross-sectional area of the reaction chamber.
 51. A preformcomprising: a) carbon; and b) at least one of a metal oxide and boricacid; wherein the carbon comprises from 10 wt. % to 35 wt. % of thepreform, and wherein the balance of the preform consists essentially ofmetal oxide(s), boric acid and combinations thereof.
 52. The preform ofclaim 51, wherein the preform at least comprises titanium dioxide andwherein the titanium dioxide comprises from 20 wt. % to 50 wt. % of thepreform.
 53. The preform of claim 52, wherein the preform at leastcomprises boric acid and wherein the boric acid comprises from 30 wt. %to 70 wt. % of the preform.
 54. The preform of claim 51, wherein thepreform comprises a plurality of granules, and wherein the preformcomprises an inter-granular porosity and an intra-granular porosity. 55.The perform of claim 51, wherein the preform is a solid, predefinedgeometric shape.